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摘 要摘要淮南煤炭资源丰富,但煤灰熔融温度高大多数F]降1500℃,无法直接应用于液态排渣的气流床气化炉。目前工业上使用的石灰石助熔剂出现频繁堵渣等问题,因而开发高效复合助熔剂具有重要的意义。本论文以淮南煤为研究对象,KZI、KZ2、KZ3和KZ4四种助熔剂为基础,利用正交配比和混料配比开发与淮南煤相适应的高效复合助熔剂,并研究高效复合助熔剂对淮南煤灰熔融特性及灰渣流动性的影响,借助X射线衍射Ⅺm分析添加高效复合助熔剂后煤灰矿物组成的变化。研究结果表明1KZ3和KZ2是影响煤灰熔融温度的主要因素,数学回归模型预测结果与验证实验结果一致。在相同的煤基添加量下,高效复合助熔剂对煤灰流动温度的降幅是KZI的2倍。同时将煤灰流动温度降至1350℃以下,高效复合助熔剂的煤基添加量是KZI的一半甚至更少。2与KZI相比,复合助熔剂可在煤基添加量减少一半时将煤灰熔融温度降至1350℃,拓宽灰渣流温区间。同时,复合助熔剂不仅添加量减少,还降低了灰渣粘度为25Pa·s时对应的温度。3由X.射线衍射分析可知高效复合助熔剂的添加破坏了煤灰中铝硅酸盐的结构,抑制了高温下莫来石的生成,随着温度的升高,出现了堇青石、长石、橄榄石和尖晶石的衍射特征峰,堇青石等低灰熔融温度的矿物与煤灰中石英等矿物在高温下发生反应,形成低熔点共熔物,从而起到降低灰熔融温度的作用。图33 表12 参76关键词气流床气化;灰熔融性;高效复合助熔剂;灰渣流动性;XRD分类号TQ53rAbstractAbstractHuainan coal is valuable,which can’t be used directly in entrained-flow BedGasification technology for its high ash fusion temperatureFT1 500“C.At present,the s used to add limestone appears frequently blocked.Therefore,it is greatsignificance to develop efficient complex flux.In this paper,four representative coalsselected from Huainan were used in the study.Orthogonal and Mixing ratio Was used todevelop efficient complex fux.Besides, effect of flux addition on Huainan coal ashfusion temperature and slag viscosity was studied.The mechanism of mineraltransation were analysed by Xray diffractionXRDwhen Effective complexflux adding.Some primary results are obtained as follows1KZ3and KZ2are important factors of the ash fusion temperature.Theresults obtained in regressive mathematical model forecast are the same as the resultsin experimental data.With the same addition of coalbased,the high effect complexflux reduced the fluidization temperature Was 2 times as high as that of KZ I.功ecoalbased addition of high effect complex flux was 0.5 times and even less as higll asthat of KZI,on condition that they could be reduced the fluidization temperaturebelow 1350℃.2Compared with KZ I,the high effect complex flux could be reduced thefluidization temperature below 1350“C when its addition Was 1/2,and not onlyextended the fluidization temperature range of ash slag,but also reduced thetemperature of 25Pa’S ash slag viscosity.3The Xray diffraction analysis shows thatThe structure of mineral phases incoals Was broken and the intensity of mullite ed Was declined at high temperame byadding efficient complex flux.With temperature increasing,the cordierite,feldspar andruby spinel phases were ed,which reacts、肮th quartz to a low-meltingeutectic mixture to lower the ash fusibility temperature.Figure 33 Table 1 2 References 76KeyWordsentrained-flow Bed Gasification,ash fusion temperature,efficient complex flux,slag fluidity,XRDChinese books catalogTQ53目 录目录摘jIj}.IAbstract..II目j;i{}IIIContents...V插图或附表清单VII弓l 言...11文献综述.21.1气流床煤气化技术的概述.21.1.1 Shell气流床煤气化技术概述.21.1.2 Texaco气流床煤气化技术概述21.2煤灰熔融特性研究现状31.2.1煤灰熔融特性与煤灰化学组成的关系.41.2.2煤灰熔融性与煤灰矿物组成的关系.51.3助熔剂的研究现状一71.3.1助熔剂在各领域的应用..71.3.2助熔剂对煤灰熔融温度的影响。71.4正交实验的应用现状81.4.1正交实验设计..81.4.2正交实验的应用现状一91.5混料实验的应用现状..101.5.1混料试验设计lO1.5.2混料实验的应用现状141.6研究内容..142实验部分1 62.1实验原料162.2煤狄熔融性实验..172.2.1制备煤灰样的实验步骤l 72.2.2灰熔融性温度测试仪器及测试方法172.2.3灰熔融性温度实验方法.182.2.4实验设备l 82.3 X一射线衍射XRD实验182.3.1制样方法1 82.3.2实验仪器l 8目 录2.4煤灰粘.温特性测试实验.192.4.1样品制备.192.4.2仪器装置193复合助熔剂对淮南煤灰熔融温度的影响研究.213.1单助熔剂对煤灰熔融温度的影响~213.1.1不同单助熔剂对煤灰熔融温度的影响213.1.2不同助熔剂对相同煤样的助熔效果比较243.1.3相同助熔剂对不同煤样的助熔效果比较253.2正交配比复合助熔剂对煤灰熔融温度的影响一263.2.1正交配比助熔剂对煤灰熔融温度的影响273.2.2 HI复合助熔剂的拓展实验.293-3混料配比复合助熔剂对煤灰熔融温度的影响.293.3.1混料配比复合助熔剂对煤灰熔融温度的影响一303.3.2最优混料配比复合助熔剂的拓展实验,353.3.3不同助熔剂对相同煤种的助熔效果比较353.4直接配比复合助熔剂对煤灰熔融温度的影响.363.4.1直接配比复合助熔剂对煤灰熔融温度的影响363.4.2不同复合助熔剂对相同煤种的助熔效果比较一393.4-3相同复合助熔剂对不同煤种的助熔效果比较一403.5小结.4l4高效复合助熔剂对淮南煤灰渣流动性的影响研究434.1复合助熔剂对淮南煤灰渣流温特性的影响研究.434.2复合助熔剂对淮南煤灰渣粘温特性的影响研究.454.3小结.455高效复合助熔剂对淮南煤的助熔机理研究475.1原煤及煤灰的XRD分析475.2高效复合助熔剂的助熔机理研究~475.3小结.53结论一54参考文献一55至l【谢..59作者简介及读研期间主要科研成果60.-IV.ContentsContents.ChiIlese AbstractIAbstractIIList of tables and figures...............................................................VIIIntroduction.................................................................................11 Literature review21.1 Entrained flow gasification technology.............................................21.2 Research progress of ash fusion characteristic....................................31.3 Research progress of fusion fluxs71.4 Application of orthogonal experiment81.5 Application of mixture experiment......................................···-······101.6 Research contents142 Experimental 162.1 Coal samples and fusion fluxs._.·162.2 Analytic ofash fusion eharacteristc172.3 Experiment of Xray diffraction182.4 Experiment of of slag viscositytemperature characteristics1 93 Effect ofcomplex flux on Huainan coal ash melting temperature....................·213.1 Effect ofpure flux on coal ash melting temperature213.2 Effect of flux on coal ash melting temperature in orthogonal ratio............263.3 Effect of flux on coal ash melting temperature in mixture ratio...............293.4 Effect of flux on coal ash melting temperature in direct ratio...............363.5 Brief summary414 Effect of efficient complex flux on the fluidity of Huainan coal ash slag............434.1 Effect of complex flux on coal ash Flow temperature characteristics434.2 Effect of complex flux on coal ash Viscosity-temperature characteristics...454.3 Brief summary..45一V-●Contents5 Mechanism of complex fusion flux on Huainan coal.................................475.1 XRD analysis of coal and coal ash................................................475.2 Mechanism of efficient complex fusion flux on Huainan coal...475.3 Brief summary........................................................................;;Conclusions.......................................................................................54Refefences.......................................................................................;;Acknowledgements..............................................................................;9Resume ofauthor.................................................................................60.VI.插图或附表清单插图或附表清单插图清单图l空间直角坐标系OXl X2X3Fig.1 Cartesian space 0-X1X2X3...............................................................................................1I 1I图2二维正规单纯形的格子点集Fig.2 Two-dimensional regular simplex ofthe lattice point set...................................................12图3二维三分量四格子点集Fig.3 Two-dimensional three-component four-frame point set...................................................12图4煤灰熔融特征温度判断Fig.4 Estimate of ash fusion temperatures..............................1 8图5 XTPRI-2型高温粘度计Fig.5 XTPRI-2 viscosimet..20图6 KZI助熔剂对不同淮南煤灰熔融特性影响的曲线图Fig.6 Relation euvres bewteen fusion temPerature and adding mount of flux KZ博.22图7 KZ3助熔剂对不同淮南煤灰熔融特性影响的曲线图Fig.7 Relation euvres bewteen fusion temPerature and adding mount of flux KZ3........22图8 KZ2助熔剂对不同淮南煤灰熔融特性影响的曲线图Fig~Relation euvres bewteen fusion temperature and adding mount of flux KZ2.23图9不同助熔剂对淮南煤助熔效果对比图Fig.9 Comparison of effect of the different flux on Huainan coal ash fusion temperature.........24图10相同助熔剂对不同淮南煤灰熔融温度影响对比图Fig.10 Comparison ofeffect ofthe same flux on Huainan coal ash fusion temperature.............2s图11正交配比助熔剂对C煤熔融特性影响柱形图Fig.1l The effect of Orthogonal ratio flux on Huainan coal ash fusiong temperature28图12 HI撑对淮南煤熔融特性影响曲线图Fig.12 Relation euvres bewteen fusion temperature and adding mount offlux HI........29图13 FT的响应曲面Fig.13 mixture surface plot of H~.33图14 FT的等值曲线Fig.14 mixture contour plot of FT......................................34图15混料设计的FT响应变量优化.V11.插图或附表清单Fig.1 5 Optimization of FT based on Mixture Design................................................................34图16 H2助熔剂对不同淮南煤熔融特性影响曲线图Fig.16 Relation eUVl 既bewteen fusion temPerature and adding mount of flux H2移35图17不同助熔剂对C煤助熔效果对比图Fig.1 7 Comparison of effect of the different flux on C coal ash fusion temperature....36图18 FHI助熔剂对不同淮南煤灰熔融特性影响的曲线图Fig.18 Relation euvr懿bewteen fusion temperature and adding mount offlux FHI..............36图19 FH2助熔剂对不同淮南煤灰熔融特性影响的曲线图Fig.19 Relation eUVl陀bewteen fusion temperature and adding mount offlux FH2...........37图20 FH3撑助熔剂对不同淮南煤灰熔融特性影响的曲线图Fig.20 Relation eUVI℃S bewteen fusion temperature and adding mount offlux FH3..............39图21相同复合助熔剂对淮南煤助熔效果对比图Fig.21 Comparison of effect of the same complex fluxes on coal ash fusion temperature.......40图22不同复合助熔剂对淮南煤的助熔效果图Fig.22 Comparison ofeffect ofthe different complex fluxes on coal ash fusion temperature......41图23 C煤4%H2复合助熔剂流温曲线Fig.23 Fluidity gDI ves of C coal by adding 4%H2flux...................................................43图24 A煤添加2%FH3复合助熔剂的流温曲线图Fig.24 Fluidity curves of A coal by adding 2%FH3撑flux~.44图25 C煤添加4%FHl复合助熔剂流温曲线Fig.25 Fluidity curves of C coal by adding 4%FH Iflux..44图26添加不同助熔剂的B煤灰粘温曲线对比图Fig.26 Comparison of slag viscosity--temperature of B coal..............................,................45图27原煤的X.射线衍射图Fig.27 XRD patters of coal samples.........................................................................................47图28 B和D煤中主要矿物衍射强度对比图Fig.28 Comparison of diffraction intensity of main minerals from coal ash samples..48图29煤灰的X一射线衍射图Fig.29 XRD patters ofash samples...........................................................................................49图30添加4%H1捍的C煤灰在不同温度下的X.射线衍射图Fig.30 XRD patters of C coal ash sample by adding H l群4%at different temperature.一50图31添加4%H1的C煤灰在在加热过程中主要矿物的强度变化插图或附表清单Fig.3 1 Mineral intensity conversion of C coal ash by adding H1撑4%.5 1图32添加4%H2的C煤灰在不同温度下的X.射线衍射图Fig.32 XRD patters of C coal ash sample by adding删l水呦at different temperature...5 1图33添加4%FHl的C煤灰在不同温度下的XRD谱图Fig.33 XRD patters of C coal ash sample by adding FH 1水哟at different temperature.52附表清单表l L423Tablel Iq2’..9表2{3,4各点坐标Table2 Three-component and four-order coordinates...............................,................................1 3表3煤样工业分析和元素分析Table3 Proximate analysis and ultimate analysis of coal samples...............................................16表4原煤煤灰化学组成叭%Table4 Ash chemical composition of coal samples....................................................................16表5煤样的灰熔融特征温度Table5 Ash fusion temperatures of coal samples........................................................................16表6L827Table6 L827~.27表7正交配比助熔剂对C煤流动温度的影响Table 7 The effect of Orthogonal ratio flux on Huainan coal ash fusion temperature.....................27表8{3,4各点坐标Table 8 Three-component and four-order coordinates................................................................30表9 C煤添加复合助熔剂的熔融特征温度Tablel0 Arrangement results of mixture design.......................................................................30袭10回归系数及影响因子的显著性分析’I’able 1 0 Regression coefficients and their significant analysis...3 1表1l C煤添加助熔剂的混料设计预测结果7I’’ablel l Predicted results ofmixture design....32表12稳定动力学参数回归模型方程的方差分析Table 12 Predicted results of mixture design...32..IX..引 言引 言随着石油、天然气资源的紧缺及洁净煤技术的发展,煤炭的地位和重要性逐渐上升。我国是世界上煤炭资源最丰富的国家之一,不仅储量大,分布广,而且煤质优良,种类齐全,全国各地拟上和新上的煤化工项目很多。安徽省发改委已经批复了安徽省煤化工淮南基地规划,计划到2020年建设成新型能源和现代煤化工生产基地。煤气化是对煤炭进行化学加工的一个重要方法,是洁净高效的煤炭综合利用技术之一,能够避免煤炭直接燃烧产生的污染。目前,先进的气流床气化工艺主要有料浆进料的湿法气化工艺Texaco水煤浆气化、多元料浆加压气化等和干煤粉进料的干法气化工艺Shell粉煤气化、GSP干粉煤气化、HT-L粉煤加压气化等,其中,Texaco和Shell等气流床气化技术以其清洁、高效代表着当今气化技术的发展潮流。气流床煤气化的优点并不仅仅在于减少空气排放物,它也生成许多具有商业价值的副产品,比如高纯度的硫、硫酸和无毒的炉渣可铺路、制砖。随着环境法的同趋严格,气流床气化的优势越来越突出。Texaco和Shell等气流床气化技术采用液态排渣,要求原料煤的灰熔融温度较低,然而我国煤炭资源分布的地理范围广泛,使得煤质有很大的差别,从而导致煤的熔融特性、粘温特性等性质差异较大。淮南矿区煤田,煤种数量较多,煤质优良,储量丰富,是优良的动力煤原料。但由于其灰熔融温度过高FT1500℃,不能直接应用于液态排渣的气流床气化炉,目前在我国已商业运行的气流床气化工艺中,普遍存在煤质不稳定,灰分含量高,灰渣熔融性不好,排渣困难等问题,.严重制约着工业化装置的安全、经济、稳定运行。解决高灰熔融温度煤直接应用于液态排渣的气流床气化炉的问题,添加助熔剂被视为经济有效的可行措施之一。助熔剂的应用较为广泛,它在钢铁、陶瓷和玻璃等制造业和材料科学等研究领域都有应用。在煤化工领域内,主要研究助熔剂对煤灰熔融特性的影响规律,降低煤灰熔融温度。煤灰的熔融特性由煤灰中矿物组成所决定,而煤灰矿物组成与煤灰化学成分有一定关系。煤灰化学组成不同,则其矿物组成不同,煤狄的熔融特性也不同。因此可以采用添加煤灰助熔剂的方式来改变煤灰化学成分,达到控制煤灰熔融特性的目的。因此,本课题研究目的在于开发适用于淮南煤气流床气化的高效复合助熔剂,这对扩大高灰熔融性煤种在气流床气化工艺中的应用,充分利用我国煤炭资源,具有重要的现实意义。
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